Water → 3-(Hydroxyphenylphosphinyl)propanoic acid

HRID 726832노트

반응식

HRID 726832 반응식
Cl[P:2](Cl)[C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1.[C:10]([O:18]OC(C)(C)C)(=[O:17])[C:11]1C=CC=C[CH:12]=1.C(O)(=[O:27])C=C.[OH2:29]>>[OH:29][P:2]([C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1)([CH2:12][CH2:11][C:10]([OH:18])=[O:17])=[O:27]

참가 물질

5

반응물 4

HCID 962WaterHCID 6581Acrylic AcidHCID 11966tert-Butyl peroxybenzoateHCID 12573Phenyl phosphorus dichloride

생성물 1

HCID 112873403-(Hydroxyphenylphosphinyl)propanoic acid

실험 절차

Using 501.2 g of dichlorophenylphosphine, 3.2 g of t-butyl peroxybenzoate, 201.8 g of acrylic acid, and 0.92 L of water, a rinse-purified 3-[hydroxy(phenyl)phosphinyl]propionic acid was prepared by the procedure described in U.S. Pat. No. 5,334,760, namely the steps of hydrolyzing the reaction mixture after completion of the reaction, cooling it, harvesting the resulting crystals by filtration, rinsing the crystal crop with water, and drying it. The yield was 564.9 g or 94.2%. From the area ratio of the respective signals on the 1H-NMR spectrum, the molar ratio of 3-[hydroxy(phenyl)phosphinyl]propionic acid to phenylphosphinic acid was found to be 99.10:0.9. The other components were traces below the detection limit.

후처리

  1. customafter completion of the reaction
  2. temperaturecooling it
  3. filtrationby filtration
  4. washrinsing the crystal crop with water
  5. customdrying it

출처 및 근거

ORD 기록
ord-672c6a8627e747fd89bac10dea930674
출처 데이터셋
uspto-grants-1998_01
특허 번호
US05710308

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